Method of preparing adsorbent and catalytic oxides



Patented Dec. 23, 1924.

UNITED STATE-SgfP'ATEN 1,520,305 r ounce.

wanna a Parisian,- or BALTIMORE, MARYLAND, ASSIGNOR TO THE small on. oonronanon, orrammoan, MARYLAND, a conroaa'rxon or marten).

: mmom or raarimnwq ansoanmrr Aim) caramz'rrcoxmas.

NoDrawing. N Application filed July 1,

To all whom it may concern." I Be it known that I, WALTER 'A. PATRICK, a citizen of the United States, and residing at Baltimore city, in the State of Maryland, have invented certain new and useful' Tm provements in Methods of Preparing Ad- 'sorbent and Catalytic Oxides, of which the followingis a specification.

The present invention relates to amethod of preparing adsorbent and-catalytic ma terials. More specifically the invention is directed to a method of producing oxides of metals Whose hydroxides are substantially insoluble in water, suchas iron, chromium, manganese, copper, bismuth, lead, thorium, nickel and vanadium, either singly .or in combination and in such physical state that they possess adsorbent and catalyticv properties. The principal aim of the invention is to produce the oxides referred to above by a method which is commercially. practicable, as distinguished from laboratory methods.

To this end the method of the presentin,

vention consists in treating a concentrated solution of a soluble salt of the aforesaid metals with a solution of a soluble alkali, such as sodium hydroxide, of such concentration and amount that after its mixture with the salt solution the resulting mixture is faintly alkaline. Preferably a very soluble salt such as a chloride is employed, and the ingredients are mixed with thorough stirring in order to prevent local heating and also for the purpose of disseminating the alkali immediately throughout the mixture to prevent excessive alkalinity inspots. .A. gelatinous precipitate, which is the hydroxide of the metal, forms immediately after the mixture of the salt and the sodium hydroxide. 1

In order to obtain a satisfactory product great care must be taken that the two' solutions, that is the salt solution and the alkaline solutions be mixed at as low a temperature as is feasible. At no timeshould the temperature be permitted to rise above about 10 C. The object of keeping the temperature low is to obtain the precipitate in a finely divided condition, this being a necessary characteristic of the product in order that it have the best adsorptive properties.

The gelatinous precipitate thus obtained is washed free of sodium chloride with 1921; Serial mag-181,990;

water. The next step consists in drying the product; To this end' the;-precipitate is firs dried 1n a stream of .airT'at to 120 C.

After this heating the {material will, still retain a considerable'quantity of water and.

the greater part of this is driven off by increasing the temperature'up to 300: to"

may, however, be dried at 120, but-this Wlll take longer. The method of" drying may be modified by taking the material after the first heating step mentioned above, and sub ect ing the same to a vacuum to further remove the water. the temperature during thls vacuum treatment being from 75 to 120 C.

By mixing solutions of. soluble salts of plurality of. said metals and sodium hydroxide or an equivalent, an adsorbent and catalytic material will be obtained, which may be termed a plural oxide. The temperature during the mixing should be kept low as already described and the precipitate 7 obtained by the mixing should be dried as previously set forth. In this manner plural oxides of vany number vor combination of sald metals maybe obtained.

What I claim as new and desire to secure by Letters Patent is: y

1. Method of preparing a highly adsorbout and catalytic oxide of a metal whose hydroxlde is substantially insoluble in water, consisting in mixing with thorough stirring a concentrated solution of a soluble salt of said metal and a solution of a soluble alkali of such concentration and amount that the resulting mixture is faintly alkaline, said mixture being maintained at a temperature not exceeding about 10 ,C., and washing and thereafter dr in the elatinous reci itate obtained. y g g v p p 2. Method of preparing a highly adsorbent and catalytic oxide of a metal Whose hy droxide is substantially insoluble in water, consisting in mixing with thorough stirring a concentrated solution of a soluble salt of said metal and a solution ofsodium hydroxide of such concentration and amount that the resulting mixture is faintly alkaline, saidmixture being maintained at a temperature not exceeding about 10 0., and washing and thereafter drying the gelatinous precipitate obtained.

3. Method of preparing a highly adsorbent and catalytic oxide of a metal Whose hydroxide is substantially insoluble in water,

' consisting. inmixing with thorough stirring a concentrated solution'of afchlor deofsai metal and a solutionof'sodiumhydroxdeof such concentration and amount' that there; 'sulting mixtureI-isfaintly alkaline,-'said' ihix5 'I tu'rebeing maintained at a;temperature}inot I A: 1exceeding smut-10 "0.; andrwashingand erea'fter dryingthe gelatinous precipitate entandI catalytic oxide 0' ametal'who'seh'y' droxideis substantially insoluble ,in" Water,

7 consisting in mixing with-ithorough stirrin a concentrated solution of'a chlor de of sai metal. and a solution of soluble alkali of such "x -concentration.and'amountthat the resulting 1 -mixture is ifaintlyalkaline, said mixture beingi maintaineds at a temperature "not; exceeding about 10C. andwashing and thereafter dryin the gelatino us', precipitate obtainedl 5.; the meth'odfof. preparing a' highly adsorbent and catalytic oxide. of a metal whose hydroxide issubstantially insoluble in 1 water; the steps vof mixing with thorough ,stirring afconc'entrated solutionlof a soluble {salt of said metal and a solution of sodiuinhydroxide v and maintaining thejresulting mixture" at. a temperature not exceeding abOutIOVCr V 6. Thednethod-of preparing vhighly ad-, Jsorhent and catalytic iron oxide, consisting. I ,in mixing with' thorough stirring a. concentrated solution Of'llOIl chloride and a 's0lu-' tion I-ofsodium hydroxideo f. such concentra- 1 x tion and amount, that the mixture is faintly alkaline, said mixture being maintained at a temperature not exceeding about 10? (land 4.;Method of'pre iarin .a'highlyiadso f rfl I H adsorbent and catalytic oxide j'offf a "meta whose hydroxid'e is I-substahtialiil insolubleat atemperature notexceedingabotit ldt G.

9. Theimethod of preparin lutionof soluble alkalijof-suclr'concentratio non!" imp ewbw qc '7 a I "7. '.the-methodlofipreparin awihighly ofv/ 'niixing .lwithqtlioroughqstirnin gaigsolug We seesaw s awsd ieb rflPil in waterythesteps of W: thorough 5 i r ng 5a so ic n iat di u cte sol e. saltof said" metal, and a solutionfof-fsolublef I alkali andmaintainingitheiresulting mixturek vi j centratedlsolution of i liloride and a so-ii. '31

and amount? that the inixture;is ;faintly -alka .hne, said mixture-being maintained-atja tem peraturewnol? exceeding about 51,09 0. "and washing and thereafter.v drying the; gelati nous preci itate obtained, 1.0.. In t e method gf pre arisgahighiy adsorbent and. catafiticfl iron'oxide the stepis 10f mixmgwith thorough stirringia' sjdlution of a"'soluble;iron;salt: and soluble alkali andgc maintaining "the resulting mixture'at aftem:

perature not exceeding about 10 7b f In testimony whereof I hereunto afiix' 

